Process for the manufacture of diethyl sulfate.



TED sra'rns r orrica LEON LILIENFELD, OF VIENNA, AUSTRIA-HUNGARY.

1,074,633. No Drawing.

Specification of Letters Patent.

Application filed May 20,

Patented Got. *7, 1913.

1913. Serial No. 768,702.

To all whom) it may concern:

Be it known that I,'LEON LILIENFELD, a subject of the Emperor of Austria-Hungary, residing at No. 1 Zeltgasse, Vienna, VIII, in theEinpire of Austria-Hungary, have invented certain new and useful Improvements in the Process for the Manufacture of Diethyl Sulfate, of which the following is a specification- This invention has for its object to provide an improved process for the manufacture of di-ethyl sulfate.

The processes proposed hitherto for the manufacture of di-ethyl sulfate have all had the drawback of giving an insuflicient yield. The best of the proposed processes whichis -'\described in the specification of German Patent No. 133,542 gives, according to the said specification, yields of 41 to 17 per cent. 4 of the theoretical quantity.

I have now discovered that di-ethyl sol; fate may be manufactured on an industrial scale and a considerably higher yield, not much below the theoretical yield, of di-ethyl sulfate may be obtained on an industrial scale, by the distillation in {000160 of sodium ethyl sulfate.

In carrying the invention into effect sodium ethyl sulfate alone or mixed with any suitable diluting agent for instance dry sul-' fate of soda, is heated, if necessary, with St11I'l11g,lI1 a vacuum, and the di-ethyl sulfate which distils over is collected in the-f usual manner in a suitable receiver. The resulting di-ethyl sulfate, if desired, may be further subjected 'to any known purifying process.

The following is an example of one way of carrying out the improved process.

Example: 1000 grams of sodium ethyl sulfate-free from water of crystallization are distilled in oa /0M0. The di-ethyl sulfate which has distilledover is mixed with cold water and extracted with chloroform. chloroform solution is drawn off, dried with calcium chlorid, filtered oil from the cal The residue consisting of pure di-ethyl sulfate weighs about from 1720 to 1870 grams. Consequently the yield of pure di-ethyl sulfate amounts to 83 to '90 per cent. of the theoretical yield, and will probably be' much higherwvhen dealing with large quantities and using specially designed apparatus.

Thecombustion of a sample of di-ethyl sulfate produced according tothe improved process gave the following results :0.2420 grams of the substance yielded (a) 0.1479 grams of H O6.78 per cent. of H.;' (6) 0.2772 grams of (10 -3123 percent. of C.

Calculated for di -ethyl sulfate H GAS per cent, (3:31.12 per cent.

1. Aprocess for the manufacture of diethyl sulfate, which consists in subjecting sodium ethyl sulfate to distillation in a vacuum. v

2. A process for the manufacture of diethyl sulfate, which consists in distilling in ooc uo sodium ethyl sulfate in mixture with a suitable diluting agent.

In testimony whereof I afiix my signature in. presence of two witnesses.

LEON LILIENFELD.

Witnesses HERMAN WUNDERLICH, FRANZ Burma.

The I cium chlorid and the chloroform driven off. 

